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Malononitrile → HCID 18319895, 화합물

HRID 1699359
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HRID 1699359 반응식
[OH-].[Na+].[C:3](#[N:7])[CH2:4][C:5]#[N:6].Cl.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17](=O)[CH:18]([NH2:20])[CH3:19])=[CH:13][CH:12]=1.C(#N)C(CC#N)O>O.C(O)C>[NH2:6][C:5]1[NH:20][C:18]([CH3:19])=[C:17]([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH3:9])=[CH:12][CH:13]=2)[C:4]=1[C:3]#[N:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8010MalononitrileHCID 14798Sodium Hydroxide2회HCID 126265652-Amino-1-(4-methoxyphenyl)propan-1-one hydrochlorideHCID 212535622-Hydroxybutanedinitrile

생성물 1

HCID 18319895HCID 18319895, 화합물수율 63.1%

시약·촉매·용매 2

HCID 702Ethanol
용매
HCID 962Water용매2회

실험 절차

To a refluxing solution (150 mL) of ethanol and water (7/3), NaOH (2.2 g, 55 mmol) and malononitrile (2.64 g, 40 mmol) were added. Then 4′-methoxy-2-aminopropiophenone hydrochloride (5.9 g, 27.2 mmol) was added in several portions. After the solution was refluxed for 30 minutes., additional malonitrile (1.3 g, 20 mmol) and NaOH (1.1 g, 27.5 mmol) were added. It was refluxed for additional 30 minutes and then poured into water (100 mL) which resulted in a precipitation. It was then filtered and washed with water until no color was washed out. The solid was then dried under vacuum at 50° C. overnight to give 2-amino-3-cyano-4-(4-methoxyphenyl)-5-methylpyrrole, (3.9 g, 63%). MS: 228 (MH+).

후처리

  1. temperatureAfter the solution was refluxed for 30 minutes
  2. temperatureIt was refluxed for additional 30 minutes
  3. customresulted in a precipitation
  4. filtrationIt was then filtered
  5. washwashed with water until no color
  6. washwas washed out
  7. customThe solid was then dried under vacuum at 50° C. overnight

출처 및 근거

ORD 기록
ord-8a4db3ceffb44f70ab945eaee80cfba7
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06346534B1

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